亚氨基-三(二甲氨基)正膦

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 5-l reactor fitted with a stirrer, a thermometer and a dropping funnel, 1.60 kg of tetrahydrofuran were weighed, followed by the addition of 250 g (1.16 mol) of aminotris(dimethylamino)phosphonium chloride. The contents were heated to 55° C., at which 2.29 kg of a 5.6 wt. % aqueous solution of barium hydroxide, said solution containing 0.83 mol (equivalent to 1.1 gram equivalents based on the chloride) of barium hydroxide, were added dropwise over 20 minutes. After completion of the dropwise addition, the resulting mixture was stirred at the same temperature for 30 minutes and was then allowed to cool down to room temperature in about 30 minutes. Iminotris(dimethylamino)phosphorane was formed with a reaction yield of 99 mol %. In a 5-l reactor fitted with a stirrer containing 0.83 mol (equivalent to 1.1 gram equivalents were added dropwise over 20 minutes After completion of the dropwise addition

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A process is provided for preparing iminotris(dimethylamino)phosphorane at high purity and high yield from aminotris(dimethylamino)phosphonium chloride. Aminotris(dimethylamino)phosphonium chloride is first reacted with an aqueous solution of the hydroxide of an alkali metal or alkaline earth metal in the presence of a solvent in which the chloride and hydroxide of the alkali metal or alkaline earth metal are sparingly soluble, whereby iminotris(dimethylamino)phosphorane is formed. After water is dissolved off at a temperature of 70° C. or lower from the reaction mixture, solids are removed from the thus-concentrated reaction mixture by solid-liquid separation. The resultant mother liquor is then distilled to obtain iminotris(dimethylamino)phosphorane.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A process is provided for preparing iminotris(dimethylamino)phosphorane at high purity and high yield from aminotris(dimethylamino)phosphonium chloride. Aminotris(dimethylamino)phosphonium chloride is first reacted with an aqueous solution of the hydroxide of an alkali metal or alkaline earth metal in the presence of a solvent in which the chloride and hydroxide of the alkali metal or alkaline earth metal are sparingly soluble, whereby iminotris(dimethylamino)phosphorane is formed. After water is dissolved off at a temperature of 70° C. or lower from the reaction mixture, solids are removed from the thus-concentrated reaction mixture by solid-liquid separation. The resultant mother liquor is then distilled to obtain iminotris(dimethylamino)phosphorane.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A process is provided for preparing iminotris(dimethylamino)phosphorane at high purity and high yield from aminotris(dimethylamino)phosphonium chloride. Aminotris(dimethylamino)phosphonium chloride is first reacted with an aqueous solution of the hydroxide of an alkali metal or alkaline earth metal in the presence of a solvent in which the chloride and hydroxide of the alkali metal or alkaline earth metal are sparingly soluble, whereby iminotris(dimethylamino)phosphorane is formed. After water is dissolved off at a temperature of 70° C. or lower from the reaction mixture, solids are removed from the thus-concentrated reaction mixture by solid-liquid separation. The resultant mother liquor is then distilled to obtain iminotris(dimethylamino)phosphorane.